Fluoroolefin/vinyl alcohol copolymer and process for its production
a technology of vinyl alcohol and copolymer, which is applied in the field of fluoroolefin/vinyl alcohol copolymer and a process for its production, can solve the problems of low reaction rate, low product quality, and low productivity, and achieve high productivity, excellent heat resistance, and prevent the effect of quality loss due to coloration
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example 1
Polymerization Step
[0080]Into a stainless steel autoclave having an internal capacity of 200 mL and equipped with a stirrer (pressure resistance: 3 MPa), 79.0 g of t-butyl alcohol, 26.7 g of t-butyl vinyl ether (hereinafter referred to as “TBVE”) as the vinyl ether (b), 0.48 g of potassium carbonate and 0.46 g of an isooctane solution containing 70% of perbutyl perpivarate (hereinafter referred to as “PBPV”) were charged, and the oxygen in the system was removed by repeating pressure purging with N2 gas. Then, 26.7 g of tetrafluoroethylene (hereinafter referred to as “TFE”) as the fluoroolefin (a) was introduced into the autoclave, followed by heating to 55° C. The pressure at that time was 1.56 MPa. Then, polymerization was continued for 7 hours, and when the pressure decreased to 1.12 MPa, the autoclave was cooled with water, and non-reacted TFE was purged to terminate the polymerization. The obtained polymer solution was put into methanol to precipitate the formed copolymer B1, f...
example 2
[0085]The copolymer B1 obtained in Example 1 was used.
[0086]Deprotection Step:
[0087]2.0 g of the copolymer B1, 50 mL of 4N hydrochloric acid and 1 mL of 1,4-dioxane were put into a 100 mL flask, heated and stirred at 90° C. to carry out a deprotection reaction. This reaction system gradually became a uniform solution. The reaction was continued for a total of 12 hours, and then, the reaction solution was dropped into water to precipitate copolymer A2, which was washed with water and then vacuum-dried at 40° C. to isolate 1.49 g of the copolymer A2.
[0088]By the measurements of the 1H-NMR spectrum and the IR spectrum, it was confirmed that in the copolymer A2, at least 97% of protective groups (t-butyl groups) were eliminated.
example 3
[0089]The copolymer B1 obtained in Example 1 was used.
[0090]Deprotection Step:
[0091]2.0 g of the copolymer B1, 50 mL of trifluoroacetic acid and 1 mL of methylene chloride were put into a 100 mL flask and then stirred at room temperature. The reaction was continued for a total of 48 hours, and then, the precipitated copolymer was washed with water and then vacuum-dried at 40° C. to isolate 1.33 g of the copolymer A3.
[0092]By the measurements of the 1H-NMR spectrum and the IR spectrum, it was confirmed that in the copolymer A3, at least 97% of protective groups (t-butyl groups) were detached.
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